EP0358088A2 - Procédé de préparation des 3-aryl-isobutanols - Google Patents

Procédé de préparation des 3-aryl-isobutanols Download PDF

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Publication number
EP0358088A2
EP0358088A2 EP89115892A EP89115892A EP0358088A2 EP 0358088 A2 EP0358088 A2 EP 0358088A2 EP 89115892 A EP89115892 A EP 89115892A EP 89115892 A EP89115892 A EP 89115892A EP 0358088 A2 EP0358088 A2 EP 0358088A2
Authority
EP
European Patent Office
Prior art keywords
propanol
formula
reaction
aryl
general formula
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
EP89115892A
Other languages
German (de)
English (en)
Other versions
EP0358088B1 (fr
EP0358088A3 (en
Inventor
Kaspar Dr. Bott
Herwig Dr. Hoffmann
Walter Dr. Scheidmeir
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
BASF SE
Original Assignee
BASF SE
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by BASF SE filed Critical BASF SE
Publication of EP0358088A2 publication Critical patent/EP0358088A2/fr
Publication of EP0358088A3 publication Critical patent/EP0358088A3/de
Application granted granted Critical
Publication of EP0358088B1 publication Critical patent/EP0358088B1/fr
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Classifications

    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C29/00Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
    • C07C29/32Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring increasing the number of carbon atoms by reactions without formation of -OH groups
    • C07C29/34Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring increasing the number of carbon atoms by reactions without formation of -OH groups by condensation involving hydroxy groups or the mineral ester groups derived therefrom, e.g. Guerbet reaction
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C33/00Unsaturated compounds having hydroxy or O-metal groups bound to acyclic carbon atoms
    • C07C33/18Monohydroxylic alcohols containing only six-membered aromatic rings as cyclic part
    • C07C33/20Monohydroxylic alcohols containing only six-membered aromatic rings as cyclic part monocyclic

Definitions

  • a generally applicable and technically preferred synthesis of the abovementioned compounds is based on the correspondingly substituted benzaldehydes, which are converted in a first stage to the corresponding 3-aryl-2-methyl-2-propenals by aldol condensation with propionaldehyde. The latter are then hydrogenated with catalytically excited hydrogen to give the corresponding saturated aldehydes or the corresponding saturated alcohols.
  • the alkyl-substituted benzaldehydes play a key role in building up the carbon structure of the above-mentioned popular fragrances and pesticide intermediates.
  • the substituted benzaldehydes are generally produced by oxidation of the corresponding alkylbenzenes - be it electrochemically, with oxygen or via halogenation - the oxi dation stage of the benzyl alcohol in question must be run through in some form. For this reason, it should be possible to make the synthesis of the 3-aryl-2-methyl-propanals of the corresponding alcohols and halides more economical if the synthesis principle used to construct the compounds mentioned could be transferred to the benzyl alcohols as starting materials.
  • the 3-aryl-isobutyl alcohols of the general formula I in the R1 and R2 are hydrogen or an alkyl or cycloalkyl radical with up to 8 carbon atoms, preferably an alkyl radical with 1 to 4 carbon atoms, in very good yields with technically acceptable conversions, if the corresponding arylcarbinols of the general formula II in the presence of catalytic amounts, ie approximately in amounts of 0.5 to 2% by weight, based on the reaction mixture, of an alkali hydroxide or an alkali alcoholate, preferably NaOH or KOH, in particular KOH, at 250 to 350 ° C. in a closed reaction vessel with n -Propanol implemented.
  • dehydrogenation catalysts such as active nickel, copper or copper bromide
  • phosphines and arsanes addition of hydrogen acceptors, such as lead salts
  • arylcarbinols of the general formula II are those in which R1 is an alkyl radical having 1 to 4 carbon atoms and R2 is H.
  • R1 is an alkyl radical having 1 to 4 carbon atoms
  • R2 is H.
  • P-methyl-benzyl alcohol, p-isopropylbenzyl alcohol and p-tert-butyl-benzyl alcohol may be mentioned in particular.
  • Alkali metal hydroxides preferably NaOH and KOH, in particular KOH, or also alkali metal alcoholates are suitable as basic catalysts.
  • the basic catalysts are used in amounts of 0.5 to 2, preferably 0.6 to 1.6% by weight, based on the reaction mixture, corresponding to about 1 to 3, preferably about 1.5 to 2.5, mol based on the Alcohols.
  • the reaction temperatures are 250 to 350 ° C, preferably 260 to 290 ° C; the reaction times about 5 to 12 hours.
  • the 3-arylisobutanols of the general formula I which are important as precursors for the wished fragrance substances jasmine orange, cyclamenaldehyde and Lysmeral® (BASF) or as intermediates for highly effective fungicides can be obtained in surprisingly good yields in a simple and economical manner.
  • the alcohols of the formula I can be converted into the fragrance substances themselves in a simple manner by oxidation with oxygen or by simple dehydrogenation.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
EP89115892A 1988-09-03 1989-08-29 Procédé de préparation des 3-aryl-isobutanols Expired - Lifetime EP0358088B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE3830019A DE3830019A1 (de) 1988-09-03 1988-09-03 Verfahren zur herstellung von 3-aryl-isobutylalkoholen
DE3830019 1988-09-03

Publications (3)

Publication Number Publication Date
EP0358088A2 true EP0358088A2 (fr) 1990-03-14
EP0358088A3 EP0358088A3 (en) 1990-05-23
EP0358088B1 EP0358088B1 (fr) 1993-06-23

Family

ID=6362253

Family Applications (1)

Application Number Title Priority Date Filing Date
EP89115892A Expired - Lifetime EP0358088B1 (fr) 1988-09-03 1989-08-29 Procédé de préparation des 3-aryl-isobutanols

Country Status (7)

Country Link
US (1) US4987270A (fr)
EP (1) EP0358088B1 (fr)
JP (1) JPH02115137A (fr)
KR (1) KR900004661A (fr)
DE (2) DE3830019A1 (fr)
ES (1) ES2055768T3 (fr)
HU (1) HU203713B (fr)

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE4447361A1 (de) * 1994-12-21 1996-06-27 Schuelke & Mayr Gmbh Biozide Alkohole, ihre Herstellung und ihre Verwendung
JP5854345B2 (ja) * 2010-03-05 2016-02-09 国立大学法人名古屋大学 二量体の製造方法
BR102019024934B1 (pt) 2019-11-26 2022-02-22 Petróleo Brasileiro S.A. - Petrobras Processo para obtenção de compostos, dentre os quais o triptano por reação de acoplamento de álcoois

Family Cites Families (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2457866A (en) * 1945-05-26 1949-01-04 Carbide & Carbon Chem Corp Condensation of alcohols
US2645667A (en) * 1951-10-01 1953-07-14 Phillips Petroleum Co Condensation of alcohols in the presence of calcium hydroxide
US3119880A (en) * 1961-05-29 1964-01-28 Gulf Research Development Co Condensation of alcohols
US3328470A (en) * 1963-10-03 1967-06-27 Continental Oil Co Greater selectivity in the guerbet reaction
NL6706692A (fr) * 1966-05-18 1967-11-20
NL6709801A (fr) * 1966-07-21 1968-01-22
DE2124589C3 (de) * 1971-05-18 1975-06-05 Basf Ag, 6700 Ludwigshafen Anthrapyrimidin-Farbstoffe und Verfahren zu ihrer Herstellung
US3860664A (en) * 1973-06-06 1975-01-14 Continental Oil Co Process for condensation of alcohols
DE3520185A1 (de) * 1985-06-05 1986-12-11 Henkel KGaA, 4000 Düsseldorf 2-benzylalkanol-1-polyglykolether sowie verfahren zu ihrer herstellung
DE3546016A1 (de) * 1985-12-24 1987-06-25 Basf Ag Verfahren zur herstellung von in 1-stellung durch aromatische oder heterocyclische reste substituierten alkanolen
DE3712873A1 (de) * 1987-04-15 1988-11-03 Consortium Elektrochem Ind 2-methyl- oder 2-methoxyphenylgruppen enthaltende alkohole und deren verwendung als duftstoffe

Also Published As

Publication number Publication date
EP0358088B1 (fr) 1993-06-23
EP0358088A3 (en) 1990-05-23
HUT51588A (en) 1990-05-28
KR900004661A (ko) 1990-04-12
JPH02115137A (ja) 1990-04-27
US4987270A (en) 1991-01-22
ES2055768T3 (es) 1994-09-01
DE3830019A1 (de) 1990-03-15
HU203713B (en) 1991-09-30
DE58904784D1 (de) 1993-07-29

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